JoVE Logo
Faculty Resource Center
Authors
Librarians
High Schools
About

Sign In

Summary

Abstract

Introduction

Protocol

Representative Results

Discussion

Acknowledgements

Materials

References

Chemistry

Mikrodalga Sentez Koşullarının Nikel Hidroksit Nano Levhaların Yapısına Etkisi

Published: August 18th, 2023

DOI:

10.3791/65412

1Materials Science, Engineering, and Commercialization Program, Texas State University, 2Department of Chemistry and Biochemistry, Texas State University, 3Westlake Highschool

Nikel hidroksit nano tabakalar, mikrodalga destekli bir hidrotermal reaksiyonla sentezlenir. Bu protokol, mikrodalga sentezi için kullanılan reaksiyon sıcaklığının ve süresinin reaksiyon verimini, kristal yapısını ve yerel koordinasyon ortamını etkilediğini göstermektedir.

Hafif asidik koşullar altında nikel hidroksit nano tabakaların hızlı, mikrodalga destekli hidrotermal sentezi için bir protokol sunulmuş ve reaksiyon sıcaklığı ve süresinin malzemenin yapısı üzerindeki etkisi incelenmiştir. İncelenen tüm reaksiyon koşulları, katmanlı α-Ni(OH)2 nano tabakaların agregaları ile sonuçlanır. Reaksiyon sıcaklığı ve süresi, malzemenin yapısını ve ürün verimini güçlü bir şekilde etkiler. α-Ni(OH)2'nin daha yüksek sıcaklıklarda sentezlenmesi reaksiyon verimini arttırır, katmanlar arası aralığı azaltır, kristal alan boyutunu arttırır, katmanlar arası anyon titreşim modlarının frekanslarını değiştirir ve gözenek çapını düşürür. Daha uzun reaksiyon süreleri, reaksiyon verimini artırır ve benzer kristal alan boyutlarına neden olur. Reaksiyon basıncının yerinde izlenmesi, daha yüksek reaksiyon sıcaklıklarında daha yüksek basınçların elde edildiğini gösterir. Bu mikrodalga destekli sentez yolu, çok sayıda enerji depolama, kataliz, sensör ve diğer uygulamalar için kullanılan çeşitli geçiş metali hidroksitlerinin sentezine ve üretimine uygulanabilen hızlı, yüksek verimli, ölçeklenebilir bir süreç sağlar.

Nikel hidroksit, Ni(OH)2, nikel-çinko ve nikel-metal hidrit piller 1,2,3,4, yakıt hücreleri4, su elektrolizörleri 4,5,6,7,8,9, süper kapasitörler4, fotokatalizörler 4, anyon değiştiriciler10 dahil olmak üzere çok sayıda uygulama için kullanılır.....

Log in or to access full content. Learn more about your institution’s access to JoVE content here

NOT: Mikrodalga sentez işleminin şematik genel bakışı Şekil 1'de sunulmuştur.

1. α-Ni(OH)2 nano tabakaların mikrodalga sentezi

  1. Öncü çözeltinin hazırlanması
    1. 15 mL ultra saf su (≥18 MΩ-cm) ve 105 mL etilen glikolü karıştırarak öncü çözeltiyi hazırlayın. 5.0 g Ni (NO3) ekleyin2 · 6H2Ove 4.1 g üre çözeltisine ve örtülür.
    2. Öncü çözeltiyi buz ve.......

Log in or to access full content. Learn more about your institution’s access to JoVE content here

Reaksiyon sıcaklığı ve süresinin α-Ni(OH)2 sentezi üzerindeki etkisi
Reaksiyondan önce, öncü çözelti [Ni(NO3)2 ·6H2O, üre, etilen glikol ve su], pH'ı 4.41 ± 0.10 olan şeffaf yeşil bir renktir (Şekil 2A ve Tablo 1). Mikrodalga reaksiyonunun sıcaklığı (120 °C veya 180 °C), çözeltinin yerinde reaksiyon basıncını ve rengini etkiler (Şekil 2B-G

Log in or to access full content. Learn more about your institution’s access to JoVE content here

Mikrodalga sentezi, geleneksel hidrotermal yöntemlere (tipik reaksiyon süreleri 4,5 saat) göre önemli ölçüde daha hızlı (13-30 dakikalık reaksiyon süresi) Ni(OH)2 üretmek için bir yol sağlar38. Ultra ince α-Ni(OH)2 nano tabakalar üretmek için bu hafif asidik mikrodalga sentez yolunu kullanarak, reaksiyon süresi ve sıcaklığının, elde edilen malzemelerin reaksiyon pH'ını, verimlerini, morfolojisini, gözenekliliğini ve yapısını etkilediği gözlemle.......

Log in or to access full content. Learn more about your institution’s access to JoVE content here

SWK ve CPR, Deniz Araştırmaları Ofisi Donanma Denizaltı Araştırma Programı'nın (Hibe No. N00014-21-1-2072) desteğini minnetle kabul eder. SWK, Deniz Araştırma Girişimi Staj Programından gelen desteği kabul eder. C.P.R ve C.M., reaksiyon koşullarının analizi için Ulusal Bilim Vakfı Malzeme Araştırma ve Eğitim Ortaklıkları (PREM) Akıllı Malzemeler Montaj Merkezi, Ödül No. 2122041'in desteğini kabul etti.

....

Log in or to access full content. Learn more about your institution’s access to JoVE content here

NameCompanyCatalog NumberComments
ATR-FTIRBrukerTensor II FT-IR spectrometer equipped with a Harrick Scientific SplitPea ATR micro-sampling accessory
Bath sonicatorFisher Scientific15-337-409--
Ethanol VWR analyticalAC61509-0040200 proof
Ethylene GlycolVWR analyticalBDH1125-4LP99% purity
Falcon Centrifuge tubesVWR analytical21008-94050 mL
KimWipesVWR analytical21905-026--
Lab Quest 2Vernier LABQ2--
Microwave ReactorAnton Parr165741Monowave 450
Ni(NO3)2 · 6 H2OWard's Science470301-856Research lab grade
pH ProbeVernier PH-BTACalibrated vs standard pH solutions (pH= 4, 7, 11)
PorosemeterMicromeritics --ASAP 2020. Analysis software: Micromeritics, version 4.03
Powder x-ray diffactometerBrukerAXS Advanced Poweder x-ray diffractometer; d-spacing, and crystallite size analyses were performed using Highscore XRD software, and crystal structures were created using VESTA 3 software.
Reaction vialAnton Parr8272330 mL G30 wideneck, 20 mL max fill capacity
Reaction vial locking lidAnton Parr161724G30 Snap Cap
Reaction vial PTFE septumAnton Parr161728Wideneck
Scanning electron microscopeFEI--Helios Nanolab 400
UreaVWR analyticalBDH4602-500GACS grade

  1. Liu, B., et al. 120 Years of nickel-based cathodes for alkaline batteries. Journal of Alloys and Compounds. 834, 155185 (2020).
  2. Young, K. H., et al. Fabrications of high-capacity α-Ni(OH)2. Batteries. 3, 6 (2017).
  3. Huang, M., Li, M., Niu, C., Li, Q., Mai, L. Recent advances in rational electrode designs for high-performance alkaline rechargeable batteries. Advanced Functional Materials. 29 (11), 1807847 (2019).
  4. Hall, D. S., Lockwood, D. J., Bock, C., MacDougall, B. R. Nickel hydroxides and related materials: a review of their structures, synthesis and properties. Proceedings of the Royal Society A. Mathematical, Physical and Engineering Sciences. 471 (2174), 20140792 (2015).
  5. Miao, Y., et al. Electrocatalysis and electroanalysis of nickel, its oxides, hydroxides and oxyhydroxides toward small molecules. Biosensors and Bioelectronics. 53, 428-439 (2014).
  6. Suen, N. T., et al. Electrocatalysis for the oxygen evolution reaction: recent development and future perspectives. Chemical Society Reviews. 46 (2), 337-365 (2017).
  7. Diaz-Morales, O., Ledezma-Yanez, I., Koper, M. T., Calle-Vallejo, F. Guidelines for the rational design of Ni-based double hydroxide electrocatalysts for the oxygen evolution reaction. ACS Catalysis. 5 (9), 5380-5387 (2015).
  8. Rossini, P. d. O., et al. Ni-based double hydroxides as electrocatalysts in chemical sensors: a review. Trends in Analytical Chemistry. 126, 115859 (2020).
  9. Yu, Z., Bai, Y., Tsekouras, G., Cheng, Z. Recent advances in Ni-Fe (Oxy)hydroxide electrocatalysts for the oxygen evolution reaction in alkaline electrolyte targeting industrial applications. Nano Select. 3 (4), 766-791 (2021).
  10. Othman, M. R., Helwani, Z., Martunus, F. W. J. N. Synthetic hydrotalcites from different routes and their application as catalysts and gas adsorbents: a review. Applied Organometallic Chemistry. 23 (9), 335-346 (2009).
  11. Bode, V. H., Dehmelt, K., Witte, J. About the nickel hydroxide electrode. II. On the oxidation products of nickel(II) hydroxidesZeitschrift für Anorganische und Allgemeine Chemie. 366, 1-21 (1969).
  12. Kimmel, S. W., et al. Capacity and phase stability of metal-substituted α-Ni(OH)2 nanosheets in aqueous Ni-Zn batteries. Materials Advances. 2 (9), 3060-3074 (2021).
  13. Corrigan, D. A., Knight, S. L. Electrochemical and spectroscopic evidence on the participation of quadrivalent nickel in the nickel hydroxide redox reaction. Journal of the Electrochemical Society. 136 (3), 613-619 (1989).
  14. Shangguan, E., et al. A comparative study of structural and electrochemical properties of high-density aluminum substituted α-nickel hydroxide containing different interlayer anions. Journal of Power Sources. 282, 158-168 (2015).
  15. Li, Y. W., et al. Effect of interlayer anions on the electrochemical performance of Al-substituted α-type nickel hydroxide electrodes. International Journal of Hydrogen Energy. 35 (6), 2539-2545 (2010).
  16. Wang, C., Zhang, X., Xu, Z., Sun, X., Ma, Y. Ethylene glycol intercalated cobalt/nickel layered double hydroxide nanosheet assemblies with ultrahigh specific capacitance: structural design and green synthesis for advanced electrochemical storage. ACS Applied Materials & Interfaces. 7 (35), 19601-19610 (2015).
  17. Hunter, B. M., Hieringer, W., Winkler, J. R., Gray, H. B., Müller, A. M. Effect of interlayer anions on [NiFe]-LDH nanosheet water oxidation activity. Energy & Environmental Science. 9 (5), 1734-1743 (2016).
  18. Zhou, D., et al. Effects of redox-active interlayer anions on the oxygen evolution reactivity of NiFe-layered double hydroxide nanosheets. Nano Research. 11, 1358-1368 (2018).
  19. Cochran, E. A., Woods, K. N., Johnson, D. W., Page, C. J., Boettcher, S. W. Unique chemistries of metal-nitrate precursors to form metal-oxide thin films from solution: materials for electronic and energy applications. Journal of Materials Chemistry A. 7 (42), 24124-24149 (2019).
  20. Bilecka, I., Niederberger, M. Microwave chemistry for inorganic nanomaterials synthesis. Nanoscale. 2 (8), 1358-1374 (2010).
  21. Zhang, X., et al. Microwave-assisted synthesis of 3D flowerlike alpha-Ni(OH)2 nanostructures for supercapacitor application. Science China Technological Sciences. 58, 1871-1876 (2015).
  22. Li, J., Wei, M., Chu, W., Wang, N. High-stable α-phase NiCo double hydroxide microspheres via microwave synthesis for supercapacitor electrode materials. Chemical Engineering Journal. 316, 277-287 (2017).
  23. Tao, Y., et al. Microwave synthesis of nickel/cobalt double hydroxide ultrathin flowerclusters with three-dimensional structures for high-performance supercapacitors. Electrochimica Acta. 111, 71-79 (2013).
  24. Zhu, Y., et al. Ultrathin nickel hydroxide and oxide nanosheets: synthesis, characterizations and excellent supercapacitor performances. Scientific Reports. 4, 1-7 (2014).
  25. Benito, P., Labajos, F. M., Rives, V. Microwave-treated layered double hydroxides containing Ni and Al: the effect of added Zn. Journal of Solid State Chemistry. 179 (12), 3784-3797 (2006).
  26. Soler-Illia, G. J. d. A., Jobbágy, M., Regazzoni, A. E., Blesa, M. A. Synthesis of nickel hydroxide by homogeneous alkalinization. precipitation mechanism. Chemistry of Materials. 11 (11), 3140-3146 (1999).
  27. Xu, L., et al. 3D flowerlike α-nickel hydroxide with enhanced electrochemical activity synthesized by microwave-assisted hydrothermal method. Chemistry of Materials. 20 (1), 308-316 (2008).
  28. Alshareef, S. F., Alhebshi, N. A., Almashhori, K., Alshaikheid, H. S., Al-Hazmi, F. A ten-minute synthesis of alpha-Ni(OH)2 nanoflakes assisted by microwave on flexible stainless-steel for energy storage devices. Nanomaterials. 12 (11), 1911 (2022).
  29. Godínez-Salomón, F., et al. Self-supported hydrous iridium-nickel oxide two-dimensional nanoframes for high activity oxygen evolution electrocatalysts. ACS Catalysis. 8 (11), 10498-10520 (2018).
  30. Godínez-Salomón, F., Albiter, L., Mendoza-Cruz, R., Rhodes, C. P. Bimetallic two-dimensional nanoframes: high activity acidic bifunctional oxygen reduction and evolution electrocatalysts. ACS Applied Energy Materials. 3 (3), 2404-2421 (2020).
  31. Ying, Y., et al. Hydrous cobalt-iridium oxide two-dimensional nanoframes: insights into activity and stability of bimetallic acidic oxygen evolution electrocatalysts. Nanoscale Advances. 3 (7), 1976-1996 (2021).
  32. Kimmel, S. W., et al. Structure and magnetism of iron-substituted nickel hydroxide nanosheets. Magnetochemistry. 9 (1), 25-47 (2023).
  33. Thommes, M., et al. Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report). Pure and Applied Chemistry. 87 (9-10), 1051-1069 (2015).
  34. Birkholz, M., Fewster, P. F., Genzel, C. . Thin Film Analysis by X-ray Scattering. , (2006).
  35. Hall, D. S., Lockwood, D. J., Poirier, S., Bock, C., MacDougall, B. R. Raman and infrared spectroscopy of alpha and beta phases of thin nickel hydroxide films electrochemically formed on nickel. Journal of Physical Chemistry A. 116 (25), 6771-6784 (2012).
  36. Choy, J. H., Kwon, Y. M., Han, K. S., Song, S. W., Chang, S. H. Intra- and inter-layer structures of layered hydroxy double salts, Ni1-xZn2x(OH)2(CH3CO2)2xnH2O. Materials Letters. 34 (3-6), 356-363 (1998).
  37. Momma, K., Izumi, F. VESTA for three-dimensional visualization of crystal, volumetric and morphology data. Journal of Applied Crystallography. 44 (6), 1272-1276 (2011).
  38. Godinez-Salomon, F., Mendoza-Cruz, R., Arellano-Jimenez, M. J., Jose-Yacaman, M., Rhodes, C. P. Metallic two-dimensional nanoframes: unsupported hierarchical nickel-platinum alloy nanoarchitectures with enhanced electrochemical oxygen reduction activity and stability. ACS Applied Materials & Interfaces. 9 (22), 18660-18674 (2017).
  39. Shakhashiri, B. Z., Dirreen, G. E., Juergens, F. Color, solubility, and complex ion equilibria of nickel (II) species in aqueous solution. Journal of Chemical Education. 57 (12), 900-901 (1980).

This article has been published

Video Coming Soon

JoVE Logo

Privacy

Terms of Use

Policies

Contact Us

Recommend to library

JoVE NEWSLETTERS

Research

Education

Authors

Librarians

ABOUT JoVE

Copyright © 2024 MyJoVE Corporation. All rights reserved